CN115073321B - Preparation method of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane - Google Patents
Preparation method of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane Download PDFInfo
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- CN115073321B CN115073321B CN202210852595.8A CN202210852595A CN115073321B CN 115073321 B CN115073321 B CN 115073321B CN 202210852595 A CN202210852595 A CN 202210852595A CN 115073321 B CN115073321 B CN 115073321B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/30—Preparation of carboxylic acid nitriles by reactions not involving the formation of cyano groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
- F26B11/02—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles
- F26B11/04—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a horizontal or slightly-inclined axis
- F26B11/0463—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a horizontal or slightly-inclined axis having internal elements, e.g. which are being moved or rotated by means other than the rotating drum wall
- F26B11/0477—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a horizontal or slightly-inclined axis having internal elements, e.g. which are being moved or rotated by means other than the rotating drum wall for mixing, stirring or conveying the materials to be dried, e.g. mounted to the wall, rotating with the drum
- F26B11/0486—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in moving drums or other mainly-closed receptacles rotating about a horizontal or slightly-inclined axis having internal elements, e.g. which are being moved or rotated by means other than the rotating drum wall for mixing, stirring or conveying the materials to be dried, e.g. mounted to the wall, rotating with the drum the elements being held stationary, e.g. internal scraper blades
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/04—Agitating, stirring, or scraping devices
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Abstract
A method for preparing 1, 4-bis [ bis (2-cyanoethyl) amino ] butane, comprising the steps of: benzyl trimethyl ammonium hydroxide is used as a catalyst, 1, 4-butanediamine and acrylonitrile are used as raw materials, water is used as a solvent, and the catalyst is prepared through reaction, filtration, washing and drying. The catalyst benzyl trimethyl ammonium hydroxide used in the application has the dosage of 5% of the dosage of 1, 4-butanediamine, the dosage is less, the catalyst benzyl trimethyl ammonium hydroxide is easy to treat and remove, the reaction speed is improved in the whole reaction, the reaction temperature is reduced, and the side reaction is reduced.
Description
Technical Field
The application relates to a preparation method of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane.
Background
Bixalomer (bisilomer) is an aminophosphoric binder developed by An Si Taylor pharmaceutical company (Astella Pharma), marketed in Japan in 2012 under the trade name Kiklin. The bisabolol is not absorbed after oral administration, and phosphate absorption is inhibited by reducing serum phosphorus concentration in the gastrointestinal tract.
1, 4-bis [ bis (2-cyanoethyl) amino ] butane is an important intermediate in the preparation of bisabolum, and has the following chemical structural formula:
the existing preparation method comprises the following steps: documents Synthetic Communications,44 (22), 3337-3345;2014. the preparation process includes the reaction of 1, 4-butanediamine with excessive acrylonitrile in the molar ratio of 1 to 8 at 80 deg.c, decompression distillation to eliminate excessive acrylonitrile and solvent water and the rest product. The product obtained by distillation in the preparation method has no crystallization process, and the purity is difficult to improve. To complete the reaction, acrylonitrile is added in excess (molar ratio 1:8), over the theoretical molar ratio (1:4) by a factor of two. Because acrylonitrile is volatile, there is leakage risk in the distillation process, causing pollution and waste. The reaction temperature is higher, 80 ℃, and the possibility of side reactions is increased. Literature "fine chemicals", 18 (7), 414-416, 420. The specific preparation process is that water is used as solvent, acetic acid is used as catalyst, 1, 4-butanediamine and a large amount of excessive acrylonitrile (molar ratio is 1:6.5) are subjected to reflux reaction, reduced pressure distillation is carried out, and the remainder is recrystallized by methanol, so that the product is obtained. According to the preparation method, the product needs to be recrystallized to improve the purity, so that the operation steps are increased, and the production process is complicated. To complete the reaction, acrylonitrile was added in large excess (molar ratio 1:6.5), exceeding the theoretical molar ratio (1:4) by 60%. There is also a risk of leakage during the distillation of acrylonitrile due to the need for distillation. The reaction temperature is higher, reflux is carried out, and the possibility of side reaction is increased.
Disclosure of Invention
In order to solve the problems, the application provides a preparation method of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane, which is characterized in that: the method comprises the following steps: benzyl trimethyl ammonium hydroxide is used as a catalyst, 1, 4-butanediamine and acrylonitrile are used as raw materials, water is used as a solvent, and the catalyst is prepared through reaction, filtration, washing and drying. The catalyst benzyl trimethyl ammonium hydroxide used in the application has the dosage of 5% of the dosage of 1, 4-butanediamine, the dosage is less, the catalyst benzyl trimethyl ammonium hydroxide is easy to treat and remove, the reaction speed is improved in the whole reaction, the reaction temperature is reduced, and the side reaction is reduced.
Preferably, the catalyst benzyl trimethyl ammonium hydroxide is preferably used in an amount of 4 to 6 weight percent of the 1, 4-butanediamine; the mol ratio of the 1, 4-butanediamine to the acrylonitrile is 1, 4-butanediamine: acrylonitrile=1:4.15-4.25; the water content of the reaction solvent is 1, 4-butanediamine (g): water (ml) =1:10-16.
Preferably, 1, 4-butanediamine, benzyltrimethylammonium hydroxide and water are put into a reaction vessel, then acrylonitrile is added dropwise at room temperature, the reaction is carried out for not less than 2 hours, filtration is carried out, the reaction vessel is washed with water for a plurality of times, and the reaction vessel is put into a drying device and dried.
Preferably, the drying device comprises a rolling cylinder, a power driving part is arranged at the side part of the rolling cylinder, a heating part is arranged at the inner side of the rolling cylinder, and a dehumidifying part is also arranged on the rolling cylinder; the rotary drum of the rolling drum body is provided with an annular inner baffle plate, a plurality of disturbance windows are arranged on the inner baffle plate, a telescopic plate is arranged in the disturbance windows, a plurality of telescopic disturbance rods are arranged below the telescopic plate, and flexible connecting strips are arranged between the telescopic plate and the inner baffle plate. The application adopts the roller body to carry out heating and dehumidifying operation, thereby realizing the drying function, avoiding internal hardening by utilizing the disturbance window on the rolling cylinder body during drying, and ensuring that the dried product can be smoothly guided out of the rolling cylinder body.
Preferably, the inner baffle is a polytetrafluoroethylene plate, a polytetrafluoroethylene outer protective layer is fixedly arranged on the inner side of the inner baffle, and folds are formed in gaps between the expansion plate and the inner baffle by the polytetrafluoroethylene outer protective layer to form flexible connecting strips; a plurality of auxiliary connecting strips made of polytetrafluoroethylene materials are further arranged between the side walls of the expansion plate and the inner baffle, and two sides of each auxiliary connecting strip are connected with the side walls of the inner baffle and the expansion plate in a thermal welding mode. The application adopts the mode of arranging the polytetrafluoroethylene outer protective layer on the inner side to fix the connecting part, and the arrangement mode of forming the flexible connecting strip on the adjacent part ensures the integration and the linkage property during operation, avoids the detachment during use and has good linkage property.
Preferably, the two sides of the rolling cylinder are respectively provided with a support bracket, the top of the support bracket is provided with a rotary bearing, and the two sides of the rolling cylinder are provided with rotary rods inserted into the rotary bearings; a material outlet is arranged on one side of the rolling cylinder body, and the height of a support bracket positioned on one side of the material outlet is lower than that of a support bracket positioned on the other side of the material outlet; the power driving part comprises a rotating motor, a driving gear is arranged at the power end of the rotating motor, a rotating gear is arranged at the outer side of the rotating rod, and a transmission chain is arranged between the rotating gear and the driving gear.
Preferably, the dehumidifying part comprises a wet guiding pipe arranged on the rotating rod, an isolated steel wire mesh is arranged in the wet guiding pipe, a negative pressure cavity is arranged on the outer side of the wet guiding pipe, and the negative pressure cavity is communicated with a negative pressure fan.
Preferably, a raw material inlet is further provided on the rolling cylinder, and an inlet cover plate is provided on the raw material inlet in a sealing manner.
Preferably, a plurality of disturbance areas consisting of disturbance windows are arranged on the inner baffle; the disturbance zone comprises 5 disturbance windows in square shapes, wherein the center points of the four disturbance windows form an arrangement square, the other disturbance window is arranged at the center of the arrangement square, and the diagonal line of each disturbance window is parallel to the diagonal line of the arrangement square; the disturbance areas are arranged according to spiral lines, the pitches of the spiral lines are the same and are 0.5-1 times of the side length of the square arrangement; the distance between the centers of adjacent disturbance areas in the spiral line direction is the same and is 2-3 times of the diagonal distance of the square. According to the application, through the design of the disturbance area, a dry dead zone is not formed in the heating process, the whole range in the rolling cylinder body can be disturbed, dead zone accumulation is avoided, the disturbance efficiency is improved, and a more optimized disturbance effect can be achieved under the condition that disturbance windows are arranged as few as possible.
Preferably, the heating part comprises a setting shaft arranged in the middle of the rolling cylinder body, and a plurality of microwave heaters are arranged on the setting shaft and face to a disturbance window in the center of the disturbance zone; the disturbance rod comprises a rod body which is arranged in the driving piston cylinder. The application adopts the design mode of the microwave heater corresponding to the disturbance window, so that the part with the best absorption can be rapidly separated, can be used as a separating parent body to drive the separation of other parts, and can avoid the overheating of the microwave heater by adding the peripheral disturbance window.
The application has the following beneficial effects: the catalyst benzyl trimethyl ammonium hydroxide used in the application has the dosage of 5% of the dosage of 1, 4-butanediamine, the dosage is less, the catalyst benzyl trimethyl ammonium hydroxide is easy to treat and remove, the reaction speed is improved in the whole reaction, the reaction temperature is reduced, and the side reaction is reduced. When drying, the application adopts the roller body to carry out heating and dehumidifying operation, thereby realizing the drying function, avoiding internal hardening by using the disturbance window on the rolling cylinder body during drying, and ensuring that the dried product can be smoothly guided out from the rolling cylinder body.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application. In the drawings:
FIG. 1 is a schematic diagram of the structure of the present application;
FIG. 2 is a schematic view of the structure with the support brackets removed;
FIG. 3 is a schematic view of the structure of a flexible connecting strip portion;
FIG. 4 is an enlarged schematic view of portion A of FIG. 1;
FIG. 5 is a schematic diagram of the structure of the disturbance zone;
fig. 6 is a schematic view of the arrangement after the rolling cylinder is deployed.
Detailed Description
In order to clearly illustrate the technical characteristics of the scheme, the application is explained in detail by the following specific embodiments.
The present application is divided into two directions, one is the preparation of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane, and one is how it is dried.
Preparation of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane:
example 1-1
A clean dry reaction vessel was charged with 44g (0.5 mol) of 1, 4-butanediamine, 1.32g of benzyltrimethylammonium hydroxide, 1320ml of purified water. 114g (2.15 mol) of acrylonitrile are added dropwise at room temperature. After the completion of the dropping, the reaction was carried out for 2 hours. The product is largely precipitated. After the completion of the thin layer detection reaction, the temperature was lowered by ice-water bath, the mixture was filtered, washed three times with purified water, and dried at 45℃by the drying apparatus in the next example to obtain 138.9g, with a purity of 99.9% and a yield of 92.5%.
Examples 1 to 2
A clean dry reaction vessel was charged with 44g (0.5 mol) of 1, 4-butanediamine, 3.52g of benzyltrimethylammonium hydroxide, 350ml of purified water. 114g (2.15 mol) of acrylonitrile are added dropwise at room temperature. After the completion of the dropping, the reaction was carried out for 2 hours, and a large amount of the product was precipitated. After the completion of the thin layer detection reaction, the temperature was lowered by ice-water bath, the reaction mixture was filtered, washed three times with purified water, and dried at 45℃by the drying apparatus of the next example to obtain 141.6g with a purity of 99.1% and a yield of 94.3%.
Examples 1 to 3
A clean dry reaction vessel was charged with 44g (0.5 mol) of 1, 4-butanediamine, 2.64g of benzyltrimethylammonium hydroxide, 700ml of purified water. 114g (2.15 mol) of acrylonitrile are added dropwise at room temperature. After the completion of the dropping, the reaction was carried out for 2 hours, and a large amount of the product was precipitated. After the completion of the thin layer detection reaction, the temperature was lowered by ice-water bath, the mixture was filtered, washed three times with purified water, and dried at 45℃by the drying apparatus in the next example to obtain 140.3g, 99.9% purity and 93.4% yield.
Examples 1 to 4
A clean dry reaction vessel was charged with 44g (0.5 mol) of 1, 4-butanediamine, 2.64g of benzyltrimethylammonium hydroxide, 530ml of purified water. 109g (2.05 mol) of acrylonitrile are added dropwise at room temperature. After the completion of the dropping, the reaction was carried out for 2 hours, and a large amount of the product was precipitated. After the completion of the thin layer detection reaction, the temperature was lowered by ice-water bath, the reaction mixture was filtered, washed three times with purified water, and dried at 45℃by the drying apparatus of the next example to obtain 141.7g with a purity of 99.5% and a yield of 94.3%.
Examples 1 to 5
A clean dry reaction vessel was charged with 44g (0.5 mol) of 1, 4-butanediamine, 2.2g of benzyltrimethylammonium hydroxide, 530ml of purified water. 111g (2.1 mol) of acrylonitrile are added dropwise at room temperature. After the completion of the dropping, the reaction was carried out for 2 hours, and a large amount of the product was precipitated. After the completion of the thin layer detection reaction, the temperature was lowered by ice-water bath, the mixture was filtered, washed three times with purified water, and dried at 45℃by the drying apparatus in the next example to obtain 143.3g, with a purity of 99.9% and a yield of 95.4%.
For the drying device, the device is originally used for drying sevelamer carbonate, but has good effect on drying 1, 4-bis [ bis (2-cyanoethyl) amino ] butane after condition selection, as shown in fig. 1-6, the drying device comprises a rolling cylinder 1, a power driving part 4 is arranged at the side part of the rolling cylinder 1, a heating part 2 is arranged at the inner side of the rolling cylinder 1, and a dehumidifying part 3 is also arranged on the rolling cylinder 1; an annular inner baffle plate 5 is arranged on the rotating cylinder wall of the rolling cylinder body 1, a plurality of disturbance windows 6 are arranged on the inner baffle plate 5, a telescopic plate 7 is arranged in the disturbance windows 6, a plurality of telescopic disturbance rods 8 are arranged below the telescopic plate 7, and flexible connecting strips 9 are arranged between the telescopic plate 7 and the inner baffle plate 5. The inner baffle 5 is a polytetrafluoroethylene plate, a polytetrafluoroethylene outer protective layer 15 is fixedly arranged on the inner side of the inner baffle 5, and the polytetrafluoroethylene outer protective layer 15 is provided with folds in gaps between the expansion plate 7 and the inner baffle 5 to form flexible connecting strips 9. A plurality of auxiliary connecting strips 10 made of polytetrafluoroethylene materials are further arranged between the side walls of the expansion plate 7 and the inner baffle 5, and two sides of each auxiliary connecting strip 10 are connected with the side walls of the inner baffle 5 and the expansion plate 7 in a thermal welding mode. The two sides of the rolling cylinder body 1 are respectively provided with a support bracket 11, the top of the support bracket 11 is provided with a rotary bearing 12, and the two sides of the rolling cylinder body 1 are provided with rotary rods 13 inserted into the rotary bearings 12; a material outlet 14 is arranged on one side of the rolling cylinder body 1, and the height of a support bracket 11 positioned on one side of the material outlet 14 is lower than that of the support bracket 11 positioned on the other side; the power driving part 4 includes a rotary motor 16, a driving gear 17 is provided at a power end of the rotary motor 16, a rotary gear 18 is provided outside the rotary lever 13, and a transmission chain 19 is provided between the rotary gear 18 and the driving gear 17. The dehumidifying part 3 comprises a moisture guiding pipe 20 arranged on a rotating rod 13, an isolating steel wire mesh 21 is arranged in the moisture guiding pipe 20, a negative pressure cavity 22 is arranged on the outer side of the moisture guiding pipe 20, and the negative pressure cavity 22 is communicated with a negative pressure fan 23. The rolling cylinder 1 is further provided with a raw material inlet 24, and the raw material inlet 24 is provided with an inlet cover plate 25 provided in a sealed manner. The inner baffle 5 is provided with a plurality of disturbance areas 26 consisting of disturbance windows 6; the disturbance zone 26 includes 5 disturbance windows 6 in a square shape, in which the center points of four disturbance windows 6 form an arrangement square, and another disturbance window 6 is provided at the center of the arrangement square, and the diagonal line of each disturbance window 6 is provided in parallel with the diagonal line of the arrangement square; the disturbance areas 26 are arranged according to a spiral line, the pitch of the spiral line is the same and is 0.5-1 times of the side length of the square arrangement; the centers of adjacent perturbation regions 26 in the spiral direction are equidistant and 2-3 times the diagonal distance of the arrangement squares. The heating part 2 comprises a setting shaft 27 arranged in the middle of the rolling cylinder 1, and a plurality of microwave heaters 28 are arranged on the setting shaft 27, wherein the microwave heaters 28 face the disturbance window 6 at the center of the disturbance zone 26. The perturbation rod 8 comprises a rod body 29, the rod body 29 being arranged into a driving piston cylinder 30.
The method comprises the following steps:
a stock solution of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane (in practice, a solid-like substance having a very high solid content) was put into the rolling cylinder 1;
the rolling cylinder 1 rotates and is heated by the heating part 2, and the expansion plate 7 on the disturbance window 6 is driven up and down by the disturbance rod 8;
and the negative pressure fan 23 is started to enable the vacuum degree of the negative pressure air cavity to reach 0.3atm, and the temperature is controlled at 45 ℃ until the preset drying condition is reached;
after the drying is finished, the negative pressure fan 23 is turned off, the heating part 2 is turned off, and the rolling cylinder 1 is continuously rotated, so that the materials in the interior are led out from the material outlet 14, and in the process, the disturbance blocks are all driven according to the rhythm of 30 times/min, and the protruding height is 5mm.
The application was tested with 1, 4-bis [ bis (2-cyanoethyl) amino ] butane having a moisture content of about 10wt% and dried to a moisture content of 2wt% (it was observed that all material was substantially free of the polytetrafluoroethylene outer protective layer 15) and placed in a device and tested with different structural forms and conditions to demonstrate the drying effect of the application.
The specific control parameters are as follows:
example 2-1
The aqueous material of example 1-1 was placed with the disturbance zone in the drum body set according to a helix with the same pitch and 0.5 times the square side length of the arrangement; the distances between the centers of adjacent disturbance areas in the spiral line direction are the same and are 3 times of the diagonal distance of the square;
when in operation, the vacuum degree of the negative pressure air cavity reaches 0.3atm, the temperature of the microwave heater is controlled to be 45 ℃; the drying time is 5.7min, and the phenomenon of adhesion with the polytetrafluoroethylene outer protective layer is avoided.
Example 2-2
The aqueous material of examples 1-2 was placed in the drum body with the disturbance zone arranged according to a helix having the same pitch and 1 time the length of the square edge of the arrangement; the distances between the centers of adjacent disturbance areas in the spiral line direction are the same and are 2 times of the diagonal distance of the square;
when in operation, the vacuum degree of the negative pressure air cavity reaches 0.3atm, the temperature of the microwave heater is controlled to be 45 ℃; the drying time is 6.2min, and the phenomenon of adhesion with the polytetrafluoroethylene outer protective layer is avoided.
Examples 2 to 3
The aqueous substances in examples 1-3 were placed in such a way that the disturbance zone in the drum body was arranged according to a spiral with the same pitch and 1 time the length of the square edge; the distances between the centers of adjacent disturbance areas in the spiral line direction are the same and are 2 times of the diagonal distance of the square;
when in operation, the vacuum degree of the negative pressure air cavity reaches 0.3atm, the temperature of the microwave heater is controlled to be 45 ℃; the drying time is 5.1min, and the phenomenon of adhesion with the polytetrafluoroethylene outer protective layer is avoided.
Examples 2 to 4
The aqueous substances of examples 1 to 4 were put into the drum body with the disturbance zone in the form of an annular arrangement, the distance between adjacent rows being 1 time the length of the sides of the arrangement square; the distance between the transversely adjacent disturbance areas is 2 times of the diagonal distance of the square;
when in operation, the vacuum degree of the negative pressure air cavity reaches 0.3atm, the temperature of the microwave heater is controlled to be 45 ℃; the drying time is 9.8min, and the phenomenon of adhesion with the polytetrafluoroethylene outer protective layer is avoided.
Examples 2 to 5
The aqueous materials of examples 1 to 5 were put into the oven, and the microwave heater was turned at an angle so as not to be set toward the disturbance block based on (2), the drying time was 11.2 minutes, and there was a phenomenon that a certain paste was stuck to the polytetrafluoroethylene outer protective layer, and after increasing the amplitude of the disturbance block by about 1 time and disturbing it by the disturbance rod for about 10 minutes, all the materials could be led out.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are to be included in the scope of the claims of the present application.
Claims (7)
1. A preparation method of 1, 4-bis [ bis (2-cyanoethyl) amino ] butane is characterized by comprising the following steps: the method comprises the following steps: benzyl trimethyl ammonium hydroxide is used as a catalyst, 1, 4-butanediamine and acrylonitrile are used as raw materials, water is used as a solvent, and the catalyst is prepared through reaction, filtration, washing and drying;
adding 1, 4-butanediamine, benzyltrimethylammonium hydroxide and water into a reaction container, then dropwise adding acrylonitrile at room temperature, reacting for at least 2 hours, filtering, washing for a plurality of times by using water, and then putting into a drying device for drying;
the drying device comprises a rolling cylinder body, a power driving part is arranged at the side part of the rolling cylinder body, a heating part is arranged at the inner side of the rolling cylinder body, and a dehumidifying part is also arranged on the rolling cylinder body; an annular inner baffle is arranged on the rotating cylinder wall of the rolling cylinder body, a plurality of disturbance windows are arranged on the inner baffle, a telescopic plate is arranged in the disturbance windows, a plurality of telescopic disturbance rods are arranged below the telescopic plate, and flexible connecting strips are arranged between the telescopic plate and the inner baffle;
a plurality of disturbance areas consisting of disturbance windows are arranged on the inner baffle; the disturbance zone comprises 5 disturbance windows in square shapes, wherein the center points of the four disturbance windows form an arrangement square, the other disturbance window is arranged at the center of the arrangement square, and the diagonal line of each disturbance window is parallel to the diagonal line of the arrangement square; the disturbance areas are arranged according to spiral lines, the pitches of the spiral lines are the same and are 0.5-1 times of the side length of the square arrangement; the distances between the centers of adjacent disturbance areas in the spiral line direction are the same and are 2-3 times of the distance between diagonal lines of the square arrangement;
the heating part comprises a setting shaft arranged in the middle of the rolling cylinder body, and a plurality of microwave heaters are arranged on the setting shaft and face to a disturbance window in the center of the disturbance zone.
2. The method for preparing 1, 4-bis [ bis (2-cyanoethyl) amino ] butane according to claim 1, wherein: the dosage of the catalyst benzyltrimethylammonium hydroxide is 4-6wt% of the dosage of the 1, 4-butanediamine; the mol ratio of the 1, 4-butanediamine to the acrylonitrile is 1, 4-butanediamine: acrylonitrile=1:4.15-4.25; the mass ratio of the 1, 4-butanediamine to the water is 1:10-16.
3. The method for preparing 1, 4-bis [ bis (2-cyanoethyl) amino ] butane according to claim 1, wherein: the inner baffle is a polytetrafluoroethylene plate, a polytetrafluoroethylene outer protective layer is fixedly arranged on the inner side of the inner baffle, and folds are formed in gaps between the expansion plate and the inner baffle by the polytetrafluoroethylene outer protective layer to form flexible connecting strips; a plurality of auxiliary connecting strips made of polytetrafluoroethylene materials are further arranged between the side walls of the expansion plate and the inner baffle, and two sides of each auxiliary connecting strip are connected with the side walls of the inner baffle and the expansion plate in a thermal welding mode.
4. The method for preparing 1, 4-bis [ bis (2-cyanoethyl) amino ] butane according to claim 1, wherein: the two sides of the rolling cylinder body are respectively provided with a support bracket, the top of the support bracket is provided with a rotary bearing, and the two sides of the rolling cylinder body are provided with rotary rods inserted into the rotary bearings; a material outlet is arranged on one side of the rolling cylinder body, and the height of a support bracket positioned on one side of the material outlet is lower than that of a support bracket positioned on the other side of the material outlet; the power driving part comprises a rotating motor, a driving gear is arranged at the power end of the rotating motor, a rotating gear is arranged at the outer side of the rotating rod, and a transmission chain is arranged between the rotating gear and the driving gear.
5. The method for preparing 1, 4-bis [ bis (2-cyanoethyl) amino ] butane according to claim 1, wherein: the dehumidifying part comprises a wet guiding pipe arranged on a rotating rod, an isolated steel wire mesh is arranged in the wet guiding pipe, a negative pressure cavity is arranged on the outer side of the wet guiding pipe, and the negative pressure cavity is communicated with a negative pressure fan.
6. The method for preparing 1, 4-bis [ bis (2-cyanoethyl) amino ] butane according to claim 1, wherein: the rolling cylinder is also provided with a raw material inlet, and the raw material inlet is provided with an inlet cover plate which is arranged in a sealing way.
7. The method for preparing 1, 4-bis [ bis (2-cyanoethyl) amino ] butane according to claim 1, wherein: the disturbance rod comprises a rod body which is arranged in the driving piston cylinder.
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